JPS63303017A - Production of w-ti alloy target - Google Patents
Production of w-ti alloy targetInfo
- Publication number
- JPS63303017A JPS63303017A JP13771087A JP13771087A JPS63303017A JP S63303017 A JPS63303017 A JP S63303017A JP 13771087 A JP13771087 A JP 13771087A JP 13771087 A JP13771087 A JP 13771087A JP S63303017 A JPS63303017 A JP S63303017A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- oxygen content
- alloy target
- titanium
- high purity
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 229910001069 Ti alloy Inorganic materials 0.000 title abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 41
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000001301 oxygen Substances 0.000 claims abstract description 31
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 31
- 239000010936 titanium Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000010894 electron beam technology Methods 0.000 claims abstract description 8
- 238000007731 hot pressing Methods 0.000 claims abstract description 8
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 8
- 229910000048 titanium hydride Inorganic materials 0.000 claims abstract description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000005520 cutting process Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 15
- 239000000956 alloy Substances 0.000 claims description 15
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 6
- 229910052721 tungsten Inorganic materials 0.000 claims description 6
- 239000010937 tungsten Substances 0.000 claims description 6
- 239000011812 mixed powder Substances 0.000 claims description 5
- -1 titanium hydride Chemical compound 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 3
- 230000001603 reducing effect Effects 0.000 abstract description 5
- 238000002844 melting Methods 0.000 abstract description 3
- 230000008018 melting Effects 0.000 abstract description 3
- 239000007789 gas Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 238000007514 turning Methods 0.000 abstract 1
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 230000004888 barrier function Effects 0.000 description 5
- 238000006356 dehydrogenation reaction Methods 0.000 description 5
- 238000009413 insulation Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000011109 contamination Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005984 hydrogenation reaction Methods 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005546 reactive sputtering Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
- Physical Vapour Deposition (AREA)
Abstract
Description
【発明の詳細な説明】
産業上の利用分野
本発明は、Ｗ−Ｔ１合金ターゲットに関するものであシ
、特には酸素含有１ｔを低減した半導体デバイス用Ｗ−
Ｔ１合金ターゲットに関する。本ターゲツ）Ｋよって、
ＩＣデバイスにおける絶縁バリアーとして使用されるＷ
−Ｔ１合金皮膜の形成が、従来よシ酸素含有量を低減し
たターゲットを使用して作製可能となり、ＩＣデバイス
の信頼性を高めることが出来る。DETAILED DESCRIPTION OF THE INVENTION Field of Industrial Application The present invention relates to a W-T1 alloy target, particularly a W-T1 alloy target with a reduced oxygen content of 1t for semiconductor devices.
Regarding T1 alloy target. This target) According to K,
W used as insulation barrier in IC devices
The -T1 alloy film can be formed using a target with a lower oxygen content than in the past, and the reliability of IC devices can be improved.
従来技術とその問題点
ＩＣデバイスにおける絶縁バリアーとしてＷ−Ｔ１
合金製皮膜を使用することは知られている。Conventional technology and its problems W-T1 as an insulation barrier in IC devices
It is known to use alloy coatings.
例えば、Ｗ−１０ｗｔ＊Ｔ１合金ターゲットを用いてＮ
鵞 雰囲気での反応性スパッタリングを利用して絶縁
バリアーを形成することが報告されている。For example, using a W-10wt*T1 alloy target, N
It has been reported that reactive sputtering in an atmosphere can be used to form an insulating barrier.
ζうしたＷ−Ｔ１合金ターゲットは、Ｗ粉末とＴ１粉末
とを混合して、粉末冶金法によ〕、即ち冷間プレス後焼
結するか或いは熱間プレスすることにより製造されてい
る。出発原料となる市販Ｔ１粉末は酸素含有量が高い。The W-T1 alloy target is manufactured by mixing W powder and T1 powder and performing cold pressing and sintering, or hot pressing. The commercially available T1 powder used as the starting material has a high oxygen content.
これは、Ｔ１は非常に活性であるため酸化し易く、表面
に不可避的に酸化膜ができるためであシ、＊ｍ＋積の大
きな粉末の場合には総酸素量はきわめて高くなる０この
ような高酸素Ｔ１粉末を原料粉末として用い粉末冶金法
によジターゲットを生成する場合、ターゲットもやはシ
酸素含有量の多いものしかできない０酸素含有量の多い
ターゲットを用いてスパッタリングを行うと、酸素の放
離によ）、ターゲットの割れ、生成皮膜の酸化、皮膜品
質のバラツキ等が生じて好ましくない。This is because T1 is very active and easily oxidized, which inevitably forms an oxide film on the surface. If the powder has a large *m+ product, the total oxygen content will be extremely high. When a ditarget is produced by powder metallurgy using high oxygen T1 powder as a raw material powder, the target has a high oxygen content.If sputtering is performed using a target with a high oxygen content, release), cracking of the target, oxidation of the formed film, variation in film quality, etc. occur, which is undesirable.
例えば、現在市販されているｗ−’ｒｉり〒ゲットは最
低限で、も１２４０ ｐｐｍの酸素を含み、多くは２５
００ ｐｐｍ乃至それ以上の酸素を含み、これでは高品
質の絶縁バリアー等の作成はできない。For example, currently commercially available w-'ri rigets contain a minimum of 1240 ppm of oxygen, and many contain 25 ppm of oxygen.
It contains 0.00 ppm or more of oxygen, and with this it is impossible to create a high quality insulation barrier.
発明の概要
とうし九斯界の実情ＫＩ！み、本発明者は、酸素含有量
を低減したＷ−Ｔｉ合金ターゲットの製造を目的として
、新たな製造方法の開発に取組んだ。Outline of the invention The actual situation in the Toushi Kyushu world KI! Therefore, the present inventor worked on the development of a new manufacturing method for the purpose of manufacturing a W-Ti alloy target with reduced oxygen content.
前述した通シ、ＴＩは、非常に活性であるなめ、Ｔ１
粉末を調製する粉砕等の工程でまたＷ粉末と混合して
成形−焼結する工程で酸素を多量にピックアップする。As previously mentioned, TI is highly active, T1
A large amount of oxygen is picked up during the pulverization process for preparing the powder, and during the molding and sintering process after mixing with the W powder.
そこで、本発明者等は、Ｔ１源として水素化チタン（Ｔ
Ｉ Ｈ，）粉末を用い、後に脱水素することを想到した
０水素化チタンを用いることのメリットは、酸化防止に
効果的であるのみならず、その喪好な粉砕性によシ酸素
ピックアップ量が減することにある。更に、脱水素の過
程で粉末の活性化効果も得られる。試行の結果、従来品
よシ酸素含有量の大巾な低減に成功した。Therefore, the present inventors investigated titanium hydride (T) as a T1 source.
The advantage of using 0-hydrogenated titanium, which is designed to be dehydrogenated later, is that it is not only effective in preventing oxidation, but also reduces the amount of oxygen pick-up due to its favorable grindability. is to decrease. Furthermore, an activation effect of the powder can be obtained during the dehydrogenation process. As a result of trials, we succeeded in significantly reducing the oxygen content compared to conventional products.
上記の知見に基いて、本発明は、タングステン（Ｗ）と
水素化チタン（ＴＩＨｓ）粉末とを混合し、生成混合粉
を脱水素後或いは脱水素しつつホットプレスすることを
特徴とするタングステン（Ｗ）−チタン（ＴＩ）合金タ
ーゲットの製造方法及び低酸素含有量（ｓ ５０〜８０
０ ｐｐｍ）のＷ−Ｔ１合金ターゲットを提供する。Based on the above findings, the present invention provides tungsten (W) and titanium hydride (TIHs) powder, which is characterized by mixing tungsten (W) and titanium hydride (TIHs) powder, and hot pressing the resulting mixed powder after or while dehydrogenating. W)-Titanium (TI) alloy target manufacturing method and low oxygen content (s 50-80
0 ppm) W-T1 alloy target.
発明の詳細な説明
Ｗ−Ｔｉ合金ターゲットは、Ｔ１を１０〜２０ｖｒｔチ
含有するＷ−Ｔ１合金製の、スパッタリング目的のター
ゲットである。ＩＣデバイスの絶縁バリアー皮膜形成目
的で上記Ｔ１含有量をとシうるが、代表的には１０ｗｔ
’ｊ 前後の’ｒＩ ｔ−含有するＷ−’ｌ’１合金が
使用されている。DETAILED DESCRIPTION OF THE INVENTION A W-Ti alloy target is a target made of a W-T1 alloy containing 10 to 20 vrt of T1 for sputtering purposes. The above T1 content can be reduced for the purpose of forming an insulation barrier film for IC devices, but typically it is 10wt.
A W-'l'1 alloy containing 'rI t- around 'j' is used.
本発明は、高純度Ｗ粉末と高純度ＴＩＭ、粉末の混合粉
を使用することを基本とする。The present invention is based on the use of a mixed powder of high-purity W powder, high-purity TIM powder, and powder.
ＴＩ Ｈ，粉末は高純度ＴＩ粉を水素化するととＫよシ
生成される。高純度ＴＩ扮を得る好ましい方法の一つは
、純度９９．９？ｗｔ−以上のスポンジチタンをエレク
トロンビーム（ＥＢ）溶解し、生成ＥＢインゴットから
切削によってＴ１切粉を生成し、これを酸洗等によシ表
面浄化することである。TI H powder is produced when high purity TI powder is hydrogenated. One of the preferred methods to obtain high purity TI filtrate is purity 99.9? The method involves melting sponge titanium of wt- or higher using electron beam (EB), cutting the produced EB ingot to produce T1 chips, and surface-purifying the chips by pickling or the like.
この方法によシ４００〜５００ ｐｐｍ酸素含有量の高
純度Ｔｉ切粉が入手しうる（Ｆ・＜ １０ ｐｐｍ ）
。By this method, high purity Ti chips with an oxygen content of 400-500 ppm can be obtained (F < 10 ppm).
.
切削は、ボール盤、セーバー、旋盤等の工作機械の任意
のものを用いて為しうるが、生産性、切粉の厚みの均−
性等の観点から旋盤の使用が好ましい。切粉の厚さは、
酸素量をなるたけ増さずに後の水素化工程が適度に進行
しうるよう２ｍ以下とするのが好ましい。更に、厚さが
大きすぎると切粉を切削しにくくなることも厚さを２−
以下とする別の理由である。厚さの下限は、かさ密度増
加、による取扱い体積の増加を考慮して（１０５■厚程
度とすることが推奨される。好ましい態様は、ａ１■±
４０’１ｇ程度に厚さを揃えることである。Cutting can be done using any machine tool such as a drill press, saver, lathe, etc., but productivity and uniformity of the thickness of the chips are important.
It is preferable to use a lathe from the viewpoint of performance etc. The thickness of the chips is
The length is preferably 2 m or less so that the subsequent hydrogenation step can proceed appropriately without increasing the amount of oxygen. Furthermore, if the thickness is too large, it will be difficult to cut chips.
This is another reason as follows. The lower limit of the thickness is recommended to be about 105cm thick, considering the increase in handling volume due to the increase in bulk density.The preferred embodiment is a1cm±
The thickness should be about 40'1g.
表面浄化は、切削時のＦ・汚染、酸化汚染等を除くため
塩酸、硫酸等の好ましくはＢＬＢ等級以上の＠を用いて
の酸洗や脱脂によシもたらされる。Surface purification is achieved by pickling and degreasing using hydrochloric acid, sulfuric acid, etc., preferably BLB grade or higher, to remove F contamination, oxidation contamination, etc. during cutting.
陶、ＥＢ溶解後のインゴットは、Ｍｇ％ＣＩ等の不純物
は除去精製されるが、Ｆｅ及び０意品位はほとんど変化
しないので、なるたけ高純度のスポンジチタンを使うこ
とが肝要である。The ingot after melting the ceramic and EB is purified to remove impurities such as Mg%CI, but the Fe and O2 grades hardly change, so it is important to use sponge titanium with as high purity as possible.
出発チタン粉末は、上記のようなＥＢ溶解−切削方法に
限定されるものでないことは云うまでも危く、例えばス
ポンジチタンの精製及びその粉砕、市販チタン粉末の精
製といった方法も採用しうる。It goes without saying that the starting titanium powder is not limited to the EB melting-cutting method as described above; for example, methods such as refining and pulverizing titanium sponge or refining commercially available titanium powder may also be employed.
こうして得られた高純度Ｔｌ粉末（切粉）の水素化はＡ
ｒ ＋ Ｈ漏気流中で３００〜５００℃の昇温下で適宜
の時間、例えば１〜５時間保持することによりもたらさ
れる。水素化は急激な水素吸収のため炉内が負圧となっ
て危険であシ、注意？：要するが、不活性ガス、％Ｋ
Ａｒ ＋ Ｈ！気流を流すことによシ急激な反応が有効
に防止できて好都合である。Hydrogenation of the high-purity Tl powder (cuttings) obtained in this way is A.
by holding at an elevated temperature of 300-500° C. for a suitable period of time, for example 1-5 hours, in an r + H leakage stream. Hydrogenation is dangerous because of the sudden hydrogen absorption, which creates negative pressure inside the furnace, so be careful! : Required, inert gas, %K
Ar+H! It is advantageous that a sudden reaction can be effectively prevented by flowing an air current.
３０〜６０チＡｒ ＋ ４０〜７０ ％ Ｈ！気流が使
用できる。生成する切粉状のＴｉＨ，ｌ不活性雰囲気（
人ｒ）中で粉砕することによ）所１５ｉ ０７Ｌ Ｈ，
粉末が得られる。粉砕は、Ｆ・及び０！汚染を抑制する
ためＡｒ中Ｍｏライニングボールミルを使用して実施す
ることが推奨される。別様にはＡｒグラブボックス内で
Ｍｏ製の乳棒及び乳鉢を用いて行なわれる。粉砕容器も
非汚染性２イニングを施したものを使用すべきである。30-60 Chi Ar + 40-70% H! Airflow is available. The generated chips of TiH, l inert atmosphere (
15i 07L H,
A powder is obtained. Grinding is F and 0! It is recommended to use a Mo-lined ball mill in Ar to reduce contamination. Alternatively, it is carried out using a Mo pestle and mortar in an Ar glove box. The crushing container should also be treated with two innings of non-contaminating material.
粉砕工程を比較的活性の少ない且つ粉砕性の良好なＴｉ
Ｈ，を用いて実施することが酸素ピックアップを最小
限とする点で大きなメリットを与える。The grinding process is carried out using Ti, which has relatively little activity and has good grindability.
Practicing with H, provides a significant advantage in minimizing oxygen pickup.
他方、Ｗ粉末は、最近アルカリ金属含有率が１００ ｐ
ｐｂ以下そして放射性元素含有率が１ｐｐｂ以下の５Ｎ
以上の高純度のものｆ：ｖ！４製する技術が確立されて
いる。これは、従来からの一般市販Ｗ或いはその化合物
音溶解して水溶ｉｔ−生成し、該水溶液を精製した後Ｗ
結晶を晶出させ、該結晶を固液分離、洗浄及び乾燥した
後に加熱還元することによって高純度Ｗ粉末を調製する
ものである。On the other hand, W powder has recently been developed with an alkali metal content of 100 p.
5N with pb or less and radioactive element content less than 1 ppb
Those with higher purity f:v! 4 technology has been established. This is a conventional general commercially available W or its compound sonodissolved to form a water-soluble it- solution, and after the aqueous solution is purified, W
High-purity W powder is prepared by crystallizing crystals, solid-liquid separation, washing, drying, and then heating reduction.
更に、これら粉末に再溶解等の精製処理を施すことによ
って更に高純度のＷ粉末を得ることができる。酸素含有
量は２００ ｐｐｍの水準にある。Further, by subjecting these powders to purification treatment such as re-dissolution, even higher purity W powder can be obtained. The oxygen content is at the level of 200 ppm.
以上のようなＴｉ Ｈ，粉末とＷ粉末とが、目標ターゲ
ット組成に応じた然るべき比率で混合される。The TiH powder and W powder as described above are mixed in an appropriate ratio depending on the target target composition.
混合は例えばＶ形ミキサを用いることによシ実施される
６ Ａｒのような不活性ガス雰囲気中で行うことが望ま
しい。しかし、若干の酸素ピックアップが起ることは避
けられない。Mixing is preferably carried out in an inert gas atmosphere such as 6 Ar, for example by using a V-mixer. However, it is inevitable that some oxygen pickup will occur.
混合物線次いで脱水素処理される。これは、Ｔｉ ａｓ
→Ｔｌ＋Ｈ意の反応に基く〇一般に６００〜７００℃の
温度において真空中又は不活性ガス中で脱水素処理は実
施される。発生する水素は、粉末表面に還元作用を及は
し、表面の活性化に寄与する。脱水素すると、０！含有
量が４００〜６００ｐｐｍ （Ｗ−１０ｗｔ％ Ｔｌの
場合）１でどうしても増大する＠
脱水素後の混合粉はホットプレスによシ成形され高密度
化される。ホットプレス条件は例えば次の通シである：
温度：１２００〜１５００℃、好ましくは１２００〜１
４００ ℃
温度が低いと密度が上らず、逆に温度が高いと酸素量が
増加する。The mixture line is then dehydrogenated. This is Ti as
→Based on the reaction Tl+H 〇 Dehydrogenation treatment is generally carried out at a temperature of 600 to 700°C in vacuum or in an inert gas. The generated hydrogen exerts a reducing action on the powder surface and contributes to surface activation. When dehydrogenated, 0! The content inevitably increases when the content is 400 to 600 ppm (in the case of W-10 wt% Tl) @ The mixed powder after dehydrogenation is molded by hot press and densified. Hot press conditions are, for example, as follows: Temperature: 1200-1500°C, preferably 1200-1
400°C If the temperature is low, the density does not increase, and conversely, if the temperature is high, the amount of oxygen increases.
圧カニ ２５０ Ｋ１７ｃｍ”以上
プレス圧は使用するダイスの耐力によって決定され、高
耐力のものが使用しうる場合には高いプレス圧を採用す
る。Pressure crab 250 K17cm" or more The press pressure is determined by the proof strength of the die used, and if a die with high proof strength can be used, a high press pressure is adopted.
時間：３０分〜２時間
プレス温度及び圧力に応じて適宜決定されるが、プレス
変位がなくなることが一つのめやすである。その後、ホ
ールドしてもよい０
雰囲気：真空（↑０−’ Ｔｏｒｒ ）別法として、上
記のように脱水素とホットプレスとを別々に行なう替Ｄ
Ｋ、同時に同じ設備を使用しても実施可能である。先ず
、Ｗ ＋ Ｔｉ Ｈｓ混合金粉末ダイケースに充填し、
１０−’ Ｔｏｒｒ 水準にまで真空引きして昇温す
る。６００〜７００℃で発生水素のために真空圧力が上
昇する。発生水素を完全に排気するよう排気に充分時間
をかけることが必要である。ダイス内から水素の抜出し
を助成する為、ガス抜き口等の配備も可能である。圧力
が再び１０”’ Ｔｑｒｒ の水準に復帰してから通
常のホットプレス操作を行なう。Time: 30 minutes to 2 hours It is determined as appropriate depending on the press temperature and pressure, but one guideline is that there is no press displacement. After that, it may be held.0 Atmosphere: Vacuum (↑0-' Torr) Alternatively, dehydrogenation and hot pressing may be performed separately as described above.
K. It is possible to carry out the same process at the same time using the same equipment. First, W + Ti Hs mixed gold powder was filled into a die case,
Evacuate to a level of 10-' Torr and raise the temperature. At 600-700°C the vacuum pressure increases due to the hydrogen generated. It is necessary to allow sufficient time for exhaust to completely exhaust the generated hydrogen. It is also possible to provide a gas vent, etc. to assist in extracting hydrogen from within the die. After the pressure has returned to a level of 10"' Tqrr, a normal hot pressing operation is carried out.
後者の同時法の方が０１含有量を一層低減しうるが、反
面水素に伴う危険性が潜在するので注意を要する。ヒー
タもＨ，との反志性を考慮してグツファイトヒータ等を
採用せねばならない。The latter simultaneous method can further reduce the 01 content, but caution is required since there is a potential danger associated with hydrogen. As for the heater, it is necessary to adopt a gutsphite heater or the like, taking into account the anti-resistance with H.
こうして、Ｗ−１０ｗｔ％ＴＩ 合金の場合、脱水素
とホットプレスを別々に行なう場合で５００〜７００
ｐｐｍ ０１含有量そして同時に行なう場合で２００〜
４００ ｐｐｍ Ｏ！含有量のホットプレス焼結体が得
られる。これを適宜機械加工することによジターゲット
が得られる。Thus, in the case of W-10 wt% TI alloy, when dehydrogenation and hot pressing are performed separately,
ppm 01 content and 200~ when done simultaneously
400 ppm O! A hot-pressed sintered body with a high content is obtained. By appropriately machining this, a ditarget can be obtained.
本方法によるターゲットは、１２４０〜２５００ｐｐｍ
の酸素含有量を有する従来ターゲットに較べ、８００
ｐｐｍ以下、代表的に３５０〜７００ ｐｐｍへと大巾
に低減された酸素含有量のものである。The target according to this method is 1240 to 2500 ppm.
Compared to a conventional target with an oxygen content of 800
The oxygen content is greatly reduced below ppm, typically 350-700 ppm.
発明の効果
Ｗ−Ｔ１合金ターゲットの酸素含有量の低減化に成功し
、酸素に伴うスパッタリング時の障害を軽減若しくは排
除し、高品質の皮！ｉＸを高い信頼性の下で形成するこ
とを可能ならしめる。Effects of the invention We succeeded in reducing the oxygen content of the W-T1 alloy target, reducing or eliminating oxygen-related obstacles during sputtering, and producing high-quality skin! It is possible to form iX with high reliability.
実施例
エレクトロンビーム溶解Ｔ１インゴットを旋盤によりＱ
ｌ−厚さに切削して得られ九Ｔｌ切粉をＡｒ５０％＋Ｈ
＊５０％気流中４００℃で３ ｈｒ 保持し、生成Ｔｉ
Ｈ，切粉ｆ：Ａｒ中で粉砕してＴｉ Ｈ，粉末全生成
した。Example Electron beam melted T1 ingot was Q
Ar50%+H
*Holded at 400℃ in 50% air flow for 3 hr to generate Ti
H, chips f: Grinded in Ar to produce TiH powder.
上記Ｔｉ Ｈ，粉末１０４０ｆとＷ粉末９０００ｆをＶ
型混合器で混合し、混合粉末を真空加熱炉へ装入した。The above TiH powder 1040f and W powder 9000f are
The mixture was mixed in a mold mixer, and the mixed powder was charged into a vacuum heating furnace.
１０”” Ｔｏｒｒ 台まで真空排気後加熱したとこ
ろ４００℃程度から炉内圧力は２ Ｔｏｒｒ まで高
くなったが６８０℃で２．５ｈｒ 保持すると再び炉
内は１０”’ Ｔｏｒｒ 台まで低くなった。冷却後
炉から取シ出し、粉末８７２１ｆｔ内径２．８６φのダ
イスに充填し、１２５０℃Ｘ ３００ Ｋ４／ｅｘ”
Ｘα５ ｈｒ の条件でホットプレスした。でき上っ
たターゲットは、密度９９．９％、酸素含有ｉ ７００
ｐｐｍであった０
比較例
市販の〒１粉末１０００ｆとＷ粉末９０００ｆをＶ型混
合器で混合し、ホットプレス用ダイスに充填した。ホッ
トプレスの条件１１１２５０℃×Ｓ ＯＯＫｐ１５＠Ｉ
Ｘα５ ｈｒ と来施例と同様とした。When the furnace was evacuated to the 10'' Torr level and then heated, the pressure inside the furnace rose to 2 Torr from around 400°C, but after being held at 680°C for 2.5 hours, the pressure in the furnace dropped to the 10'' Torr level again. Cooling. Take out the powder from the after-furnace, fill it into a die with 8721ft of powder and an inner diameter of 2.86φ, and heat it at 1250°C x 300 K4/ex”
Hot pressing was carried out under the conditions of Xα5 hr. The finished target has a density of 99.9% and an oxygen content of 700
ppm was 0.Comparative Example 1000f of commercially available 〒1 powder and 9000f of W powder were mixed in a V-type mixer and filled into a hot press die. Hot press conditions 111250℃×S OOKp15@I
Xα5 hr was the same as in the next example.
密度は９９．９チであったが酸素含有量は１５００ｐｐ
ｍであったＯ
同 風間弘志゛３
゛・ヲThe density was 99.9 inches, but the oxygen content was 1500pp.
M was O Same Hiroshi Kazama゛゛3 ゛・wo
Claims (1)
２）粉末とを混合し、生成混合粉を脱水素後或いは脱水
素しつつホットプレスすることを特徴とするタングステ
ン（Ｗ）−チタン（Ｔｉ）合金ターゲットの製造方法。 ２）水素化チタン粉末が高純度チタンのエレクトロンビ
ーム溶解インゴットを切削して得られる切粉を（Ａｒ＋
Ｈ＿２）気流中で加熱して水素化しその後粉砕すること
により生成される特許請求の範囲第１項記載の方法。 ３）酸素含有量が３５０〜８００ｐｐｍであることを特
徴とするタングステン（Ｗ）−チタン（Ｔｉ）合金ター
ゲット。[Claims] 1) Tungsten (W) powder and titanium hydride (TiH_
2) A method for producing a tungsten (W)-titanium (Ti) alloy target, which comprises mixing the tungsten (W)-titanium (Ti) alloy target with powder and hot pressing the resulting mixed powder after dehydrogenating or while dehydrogenating. 2) Titanium hydride powder cuts chips obtained by cutting an electron beam melted ingot of high purity titanium (Ar+
H_2) The method according to claim 1, which is produced by heating in an air stream to hydrogenate and then pulverizing. 3) A tungsten (W)-titanium (Ti) alloy target characterized by having an oxygen content of 350 to 800 ppm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13771087A JPS63303017A (en) | 1987-06-02 | 1987-06-02 | Production of w-ti alloy target |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13771087A JPS63303017A (en) | 1987-06-02 | 1987-06-02 | Production of w-ti alloy target |
Related Child Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5317470A Division JP2610575B2 (en) | 1993-11-25 | 1993-11-25 | W-Ti alloy target |
| JP32088093A Division JPH0711434A (en) | 1993-11-29 | 1993-11-29 | W-ti alloy target |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63303017A true JPS63303017A (en) | 1988-12-09 |
| JPH05452B2 JPH05452B2 (en) | 1993-01-06 |
Family
ID=15205013
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP13771087A Granted JPS63303017A (en) | 1987-06-02 | 1987-06-02 | Production of w-ti alloy target |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63303017A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03264640A (en) * | 1990-03-13 | 1991-11-25 | Hitachi Metals Ltd | Ti-w target material and production thereof |
| JPH04232260A (en) * | 1990-12-28 | 1992-08-20 | Nikko Kyodo Co Ltd | W-ti alloy target and its manufacture |
| US5160534A (en) * | 1990-06-15 | 1992-11-03 | Hitachi Metals Ltd. | Titanium-tungsten target material for sputtering and manufacturing method therefor |
| US5298338A (en) * | 1990-06-15 | 1994-03-29 | Hitachi Metals, Ltd. | Titanium-tungsten target material and manufacturing method thereof |
| US5306569A (en) * | 1990-06-15 | 1994-04-26 | Hitachi Metals, Ltd. | Titanium-tungsten target material and manufacturing method thereof |
| JP2002339031A (en) * | 2001-05-16 | 2002-11-27 | Allied Material Corp | Molybdenum sputtering target and manufacturing method |
| CN102366833A (en) * | 2011-11-21 | 2012-03-07 | 宁波江丰电子材料有限公司 | Production method of tungsten-titanium target blank |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS49103810A (en) * | 1973-02-07 | 1974-10-01 | ||
| JPS5027706A (en) * | 1973-07-13 | 1975-03-22 | ||
| JPS5249915A (en) * | 1975-10-20 | 1977-04-21 | Hitachi Metals Ltd | Production process of sintered alloy containing titanium |
| US4331476A (en) * | 1980-01-31 | 1982-05-25 | Tektronix, Inc. | Sputtering targets with low mobile ion contamination |
| JPS6066425A (en) * | 1983-09-22 | 1985-04-16 | Nippon Telegr & Teleph Corp <Ntt> | High-purity molybdenum target and high-purity molybdenum silicide target for lsi electrode and manufacture thereof |
| JPS6158866A (en) * | 1984-08-30 | 1986-03-26 | 三菱マテリアル株式会社 | Manufacture of high melting point metal silicate base composite material |
-
1987
- 1987-06-02 JP JP13771087A patent/JPS63303017A/en active Granted
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS49103810A (en) * | 1973-02-07 | 1974-10-01 | ||
| JPS5027706A (en) * | 1973-07-13 | 1975-03-22 | ||
| JPS5249915A (en) * | 1975-10-20 | 1977-04-21 | Hitachi Metals Ltd | Production process of sintered alloy containing titanium |
| US4331476A (en) * | 1980-01-31 | 1982-05-25 | Tektronix, Inc. | Sputtering targets with low mobile ion contamination |
| JPS6066425A (en) * | 1983-09-22 | 1985-04-16 | Nippon Telegr & Teleph Corp <Ntt> | High-purity molybdenum target and high-purity molybdenum silicide target for lsi electrode and manufacture thereof |
| JPS6158866A (en) * | 1984-08-30 | 1986-03-26 | 三菱マテリアル株式会社 | Manufacture of high melting point metal silicate base composite material |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03264640A (en) * | 1990-03-13 | 1991-11-25 | Hitachi Metals Ltd | Ti-w target material and production thereof |
| US5160534A (en) * | 1990-06-15 | 1992-11-03 | Hitachi Metals Ltd. | Titanium-tungsten target material for sputtering and manufacturing method therefor |
| US5298338A (en) * | 1990-06-15 | 1994-03-29 | Hitachi Metals, Ltd. | Titanium-tungsten target material and manufacturing method thereof |
| US5306569A (en) * | 1990-06-15 | 1994-04-26 | Hitachi Metals, Ltd. | Titanium-tungsten target material and manufacturing method thereof |
| JPH04232260A (en) * | 1990-12-28 | 1992-08-20 | Nikko Kyodo Co Ltd | W-ti alloy target and its manufacture |
| JP2002339031A (en) * | 2001-05-16 | 2002-11-27 | Allied Material Corp | Molybdenum sputtering target and manufacturing method |
| CN102366833A (en) * | 2011-11-21 | 2012-03-07 | 宁波江丰电子材料有限公司 | Production method of tungsten-titanium target blank |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH05452B2 (en) | 1993-01-06 |
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